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1.
以硫羟硫胺为原料,经双氧水氧化得硫酸维生素B1(VB1·H2SO4);VB1·H2SO4经纯化水稀释后,流经732强酸型阳离子交换树脂,用稀盐酸洗脱,浓缩后用85%乙醇重结晶得盐酸VB1,其结构经1H NMR,13C NMR,MS和元素分析确证。 相似文献
2.
New and convergent synthetic route of osimertinib is described on a dozen of grams scale. A key cyclization of 1‐(4‐((2‐(dimethylamino)ethyl)(methyl)amino)‐2‐methoxy‐5‐nitrophenyl)guanidine and 3‐(dimethylamino)‐1‐(1‐methyl‐1 H‐indol‐3‐yl)prop‐2‐en‐1‐one is adopted to give the 4‐(1 H‐indol‐3‐yl)‐ N‐phenylpyrimidin‐2‐amine structure. Osimertinib is prepared in 40.4% yield over six steps and 99.1% purity (HPLC). Purification methods of the intermediates involved in the route are also given. 相似文献
3.
A simple and efficient one-pot synthesis of 1 H-benzimidazole derivatives using thiamine hydrochloride (VB 1) as the organocatalyst from o-phenylenediamine and aldehyde in dimethylformamide is described. Compared to classical reaction conditions, this new method consistently has the advantages of excellent yields, metal-ion-free procedure, and good recovery and reusablity of catalyst. 相似文献
4.
Abstract A concise synthesis of sarmentosin ( 1) starting from butane-1,2,4-triol-1,2-acetonide is described. This convergent route can also be employed for the preparation of sarmentosin analogues for structure-activity relationship studies. 相似文献
6.
以邻氨基苯甲酸甲酯(1)为起始原料,与溴素发生溴化反应制得2-氨基-3,5-二溴苯甲酸甲酯(2)。2经红铝试剂还原制得2-氨基-3,5-二溴苯甲醛(3); 3经还原胺化制得氨溴索(4); 4盐酸化得到盐酸氨溴索(5),总收率60.8%,其结构经 1H NMR确证。 相似文献
9.
Difloxacin, the third generation of new quinolone antibiotics, has broad-spectrum in vitro activity and excellent potency in vivo and has been found to be against gram-positive cocci, gram-negative bacteria, anaerobe, mycoplasm, chlamydia1,2. As described previously, high reaction temperature and hazardous reagents are the defects of the methods for preparation of difloxacin3,4. We have developed a new synthetic method as shown in the Scheme. 2,4-Dichloro-5-fluoro-acetophenone 1 was used as … 相似文献
10.
A short, convergent synthesis of (±) patulolide A, a 12-membered macrolide with high antifungal activities is hereby reported. It has been achieved in 10 steps from 1-bromopentanal and 4-hydroxypent-1-yne. 相似文献
11.
Abstract A short, convenient, and efficient synthesis of 4-nitrophenethylamine hydrochloride is described. The key step involved removal of water from 4-nitrophenylalanine monohydrate followed by decarboxylation. 相似文献
12.
AF-5 was synthesized through a convergent method. The key step was the Robinson annulation using a key intermediate pentyl vinyl ketone. 相似文献
15.
(R)-1-萘乙胺与丙烯酰氯发生亲核取代反应制得酰胺(2); 2与3-三氟甲基碘苯经Heck偶联反应制得α,β-不饱和酰胺(3); 3经两次还原反应后再与盐酸成盐合成了盐酸西那卡塞,总收率40%,纯度>99.5%, ee值>99.9%,其结构经 1H NMR和 13C NMR确证。 相似文献
16.
A convergent approach to dibenzodioxocinones was explored, thereby racemic penicillide ((±)‐ 1a ) could be obtained in 13 steps in 4.2% overall yield, based on 5‐amino‐2‐methylphenol ( 5 ) ( Schemes 2–4). 相似文献
17.
Abstract—Electronic interactions associated with charge transfer complexes formation of iodine, chloranilic acid (H2CA) and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) with vitamin B1 have been studied spectrophotometrically. The accumulated data indicated formation of CT-complexes of the general formula [(VB1)(acceptor)
n
], (n = 1 or 2). The 1 : 2 and 1 : 1 donor: acceptor molar ratios were calculated on the basis of elemental analysis and photometric titrations. The solid complexes were prepared and characterized by their conductivity, UV-Vis, IR, and 1H NMR spectra, and thermogravimetric analyses (TGA, DTG). The characteristic physical constants (KCT, εCT, μ, ΔG, Ip, f, ECT) of the formed CT-complexes were determined to be strongly dependent on nature of the electron acceptors. 相似文献
18.
以3-氯苯丙酮为起始原料,经不对称还原、烃化、O-甲磺酰化、SN2二甲胺化和成盐合成了盐酸达泊西汀,总收率39.9%,其结构经1H NMR和MS确证. 相似文献
19.
以N,N′-二甲基脲为原料,经氰乙酸环合、乙醇胺脱氨、二氯亚砜氯化3步反应合成了关键中间体6-(2-氯乙基)胺基-1,3-二甲基-嘧啶二酮(7)。7再与:N-(2-羟乙基)-3-(4-硝基苯基)丙胺反应得抗心律失常药盐酸尼非卡兰,总收率为48.0%(以N,N′-二甲基脲计),其结构经NMR和MS确认。 相似文献
20.
以对羟基苯乙酸和苯酞为原料,经缩合、环合、Wittig反应等合成了抗过敏药盐酸奥洛他定,总收率12.5%,其结构经1H NMR, IR和MS确证. 相似文献
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